CN109336174A - A kind of method that molten-salt growth method prepares bismuth titanates nanometer rods - Google Patents

A kind of method that molten-salt growth method prepares bismuth titanates nanometer rods Download PDF

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CN109336174A
CN109336174A CN201811487968.6A CN201811487968A CN109336174A CN 109336174 A CN109336174 A CN 109336174A CN 201811487968 A CN201811487968 A CN 201811487968A CN 109336174 A CN109336174 A CN 109336174A
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bismuth
solution
nanometer rods
molten
bismuth titanates
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CN109336174B (en
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杨琳琳
陈建
王永刚
阳勇福
王玉江
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Luoyang Institute of Science and Technology
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Luoyang Institute of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G29/00—Compounds of bismuth
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

Abstract

The invention discloses a kind of methods that molten-salt growth method prepares bismuth titanates nanometer rods, first prepare the oxyhydroxide precipitation solution of bismuth, then it is mixed with titanium sulfate solution, drying after mixed precipitation solution ultrasonication is obtained into presoma again, presoma and sodium chloride grinding is uniform, gained mixture is put in crucible, and crucible is placed in electric furnace heat preservation 1h~3h under the conditions of 820~950 DEG C, takes out cooling；It is dried after finally cooling sample is cleaned, that is, obtains the bismuth titanates nanometer rods powder of well-crystallized.The present invention has simple process; the size of nano-powder is easy to control; it is low in cost; do not use organic surface active agent; it is pollution-free, it is easy to accomplish the advantages of large-scale production, the bismuth titanates nanometer rods prepared are because of its unique club shaped structure; in fields such as photocatalysis, sensor, capacitor, display, infrared detector, piezoelectricity conversion, memory, microelectron-mechanicals, there is more excellent performance and broad application prospect.

Description

A kind of method that molten-salt growth method prepares bismuth titanates nanometer rods
Technical field
The invention belongs to field of inorganic nonmetallic material, and in particular to a kind of molten-salt growth method prepares the side of bismuth titanates nanometer rods Method.
Background technique
Bismuth titanates (Bi4Ti3O12) it is a kind of very important functional material, in photocatalysis, sensor, capacitor, display The fields such as device, infrared detector, piezoelectricity conversion, memory, microelectromechanical systems have a wide range of applications.The preparation of bismuth titanates Method can be divided into solid reaction process and wet chemical method, and solid phase method preparation needs higher temperature, and the product generated is reunited Seriously, pattern is difficult to control.Wet chemical method has colloidal sol~gel method, hydro-thermal method, coprecipitation etc., although these methods can be with Bismuth titanates is synthesized at a lower temperature, but obtained bismuth titanates pattern is still uneven, is unable to control its size.And these What method prepared is usually the bismuth titanates of sheet.Prepared by hydro-thermal method usually requires addition surface modification in the technique of bismuth titanates Agent causes the post-processing of product pretty troublesome.
The preparation method about the nano bar-shape bismuth titanates of pattern uniform, controllable is rarely reported at present.It is well known that having The nano crystal material of special appearance often shows some excellent performances, therefore, prepares the bismuth titanates of novel in shape It all has very important significance in terms of the resonable opinion basic research of nanometer rods crystal and practical application.
Summary of the invention
The object of the present invention is to provide a kind of simple process, morphology controllable, the low in cost, fused salts that are easily industrialized The method that method prepares bismuth titanates nanometer rods, prepared bismuth titanates nanometer rods are urged because of its unique one-dimensional rod-like structure in light The fields such as change, sensor, capacitor, display, infrared detector, piezoelectricity conversion, memory, microelectromechanical systems, have More excellent performance has more broad application prospect.
The object of the invention to solve the technical problems adopts the following technical solutions to realize.
The method that a kind of molten-salt growth method proposed according to the present invention prepares bismuth titanates nanometer rods comprising following steps:
Step 1: titanium sulfate is made into aqueous solution, the concentration for adjusting the titanium ion in solution is 0.03~0.8mol/L；
Step 2: bismuth nitrate is dissolved in the dilute nitric acid solution that mass concentration is 5%, the dense of the bismuth ion in solution is adjusted Degree is 0.04~1.0mol/L；
Step 3: bismuth nitrate solution made from step 2 and excessive potassium hydroxide aqueous solution are mixed, after making mixing Solution pH value be 14, obtain the oxyhydroxide precipitation solution of bismuth, this precipitation solution and titanium sulfate made from step 1 is molten Liquid mixing, wherein the molar ratio of bismuth ion and titanium ion is 4:3, and mixed precipitation solution is with 20~40 points of ultrasonic echography Clock, ultrasonic frequency are 1000~2000W, dry obtained precipitation solution to obtain presoma later；
Step 4: presoma made from step 3 and the solid sodium chloride as fused salt are fully ground, gained mixture It is placed in corundum crucible, then crucible is put into electric furnace, after keeping the temperature 1h~3h under the conditions of 820~950 DEG C, take out, it is cooling；
Step 5: being dried after sample after cooling is cleaned with deionized water to get the bismuth titanates nanometer of well-crystallized is arrived Stick.The object of the invention to solve the technical problems also can be used following technical measures and further realize.
The method that molten-salt growth method above-mentioned prepares bismuth titanates nanometer rods, wherein presoma and sodium chloride when being ground in step 4 Weight ratio be 1:2~1:10.
The method that molten-salt growth method above-mentioned prepares bismuth titanates nanometer rods, wherein bismuth nitrate, titanium sulfate and the potassium hydroxide Purity be not less than chemistry it is pure.
The method that molten-salt growth method above-mentioned prepares bismuth titanates nanometer rods, wherein the length of gained bismuth titanates nanometer rods be 300~ 600nm, diameter are about 30~80nm.
The method that molten-salt growth method above-mentioned prepares bismuth titanates nanometer rods, wherein gained bismuth titanates nanometer rods are used to prepare light and urge Change material, sensor material, capacitor material, piezoelectricity transition material, microelectron-mechanical material etc..
The beneficial effects of the present invention are:
The present invention has prepared good crystallinity (crystallinity is greater than 96%), purity is high using molten-salt growth method (purity is greater than 99%) Bismuth titanates nanometer rods powder, the length of single nanometer rods is about 300~600nm, and diameter is about 30~80nm, and nanometer rods Size can by change technological parameter be adjusted.The method that molten-salt growth method of the invention prepares bismuth titanates nanometer rods powder, Have many advantages, such as equipment is simple, technique rapidly and efficiently, condition be easy to control, prepare low in cost, and the present invention does not use Any organic surface active agent or coating material are not necessarily to post-processing, non-environmental-pollution, easy to industrialized production.The present invention The middle bismuth titanates nanometer rods prepared using molten-salt growth method are because of its unique one-dimensional rod-like structure, in photocatalysis, sensor, capacitor The fields such as device, display, infrared detector, piezoelectricity conversion, memory, microelectromechanical systems have more excellent performance, There is more broad application prospect.
Detailed description of the invention
Fig. 1 is the XRD spectrum for the bismuth titanates nanometer rods that the present invention synthesizes；
Fig. 2 is transmission electron microscope (TEM) photo for the bismuth titanates nanometer rods that the present invention synthesizes；
Specific embodiment
It is of the invention to reach the technical means and efficacy that predetermined goal of the invention is taken further to illustrate, below in conjunction with Attached drawing and preferred embodiment, it is specific real to a kind of method that molten-salt growth method prepares bismuth titanates nanometer rods proposed according to the present invention Mode, structure, feature and its effect are applied, detailed description is as follows.
Embodiment 1
Step 1: titanium sulfate is made into aqueous solution, the concentration for adjusting the titanium ion in solution is 0.03mol/L；
Step 2: bismuth nitrate is dissolved in the dilute nitric acid solution that mass concentration is 5%, the dense of the bismuth ion in solution is adjusted Degree is 0.04mol/L；
Step 3: bismuth nitrate solution made from step 2 and excessive potassium hydroxide aqueous solution are mixed, after making mixing Solution pH value be 14, obtain the oxyhydroxide precipitation solution of bismuth, this precipitation solution and titanium sulfate made from step 1 is molten Liquid mixing, wherein the molar ratio of bismuth ion and titanium ion is 4:3, and mixed precipitation solution was surpassed with ultrasonic echography 20 minutes Frequency of sound wave is 1000W, dries obtained precipitation solution to obtain presoma later；
Step 4: presoma made from step 3 and the solid sodium chloride as fused salt are fully ground, wherein presoma Weight ratio with sodium chloride is 1:2, and grinding gained mixture is placed in corundum crucible, then crucible is put into electric furnace, at 820 DEG C Under the conditions of keep the temperature 3h after, take out, it is cooling；
Step 5: being dried after sample after cooling is cleaned with deionized water to get the bismuth titanates nanometer of well-crystallized is arrived Stick, the length of single nanometer rods are about 300~400nm, and diameter is about 30~50nm.Its XRD spectrum is shown in Fig. 1；Transmission electron microscope picture See Fig. 2.Fig. 1 and Fig. 2 shows that the method for the present invention is not introduced into impurity, obtained titanium during preparing bismuth titanates nanometer rods Sour bismuth nanometer rods crystal crystallinity is good, and pattern is uniform.
Embodiment 2
Step 1: titanium sulfate is made into aqueous solution, the concentration for adjusting the titanium ion in solution is 0.3mol/L；
Step 2: bismuth nitrate is dissolved in the dilute nitric acid solution that mass concentration is 5%, the dense of the bismuth ion in solution is adjusted Degree is 0.4mol/L；
Step 3: bismuth nitrate solution made from step 2 and excessive potassium hydroxide aqueous solution are mixed, after making mixing Solution pH value be 14, obtain the oxyhydroxide precipitation solution of bismuth, this precipitation solution and titanium sulfate made from step 1 is molten Liquid mixing, wherein the molar ratio of bismuth ion and titanium ion is 4:3, and mixed precipitation solution was surpassed with ultrasonic echography 30 minutes Frequency of sound wave is 2000W, dries obtained precipitation solution to obtain presoma later；
Step 4: presoma made from step 3 and the solid sodium chloride as fused salt are fully ground, wherein presoma Weight ratio with sodium chloride is 1:6, and grinding gained mixture is placed in corundum crucible, then crucible is put into electric furnace, at 900 DEG C Under the conditions of keep the temperature 2h after, take out, it is cooling；
Step 5: being dried after sample after cooling is cleaned with deionized water to get the bismuth titanates nanometer of well-crystallized is arrived Stick, the length of single nanometer rods are about 400~500nm, and diameter is about 40~60nm.
Embodiment 3
Step 1: titanium sulfate is made into aqueous solution, the concentration for adjusting the titanium ion in solution is 0.6mol/L；
Step 2: bismuth nitrate is dissolved in the dilute nitric acid solution that mass concentration is 5%, the dense of the bismuth ion in solution is adjusted Degree is 0.8mol/L；
Step 3: bismuth nitrate solution made from step 2 and excessive potassium hydroxide aqueous solution are mixed, after making mixing Solution pH value be 14, obtain the oxyhydroxide precipitation solution of bismuth, this precipitation solution and titanium sulfate made from step 1 is molten Liquid mixing, wherein the molar ratio of bismuth ion and titanium ion is 4:3, and mixed precipitation solution was surpassed with ultrasonic echography 40 minutes Frequency of sound wave is 1500W, dries obtained precipitation solution to obtain presoma later；
Step 4: presoma made from step 3 and the solid sodium chloride as fused salt are fully ground, wherein presoma Weight ratio with sodium chloride is 1:10, and grinding gained mixture is placed in corundum crucible, then crucible is put into electric furnace, 950 After keeping the temperature 1h under the conditions of DEG C, take out, it is cooling；
Step 5: being dried after sample after cooling is cleaned with deionized water to get the bismuth titanates nanometer of well-crystallized is arrived Stick, the length of single nanometer rods are about 500~600nm, and diameter is about 60~80nm.
The above described is only a preferred embodiment of the present invention, being not intended to limit the present invention in any form, appoint What those skilled in the art, it is without departing from the scope of the present invention, all without departing from technical solution of the present invention Content, any simple modification, equivalent change and modification to the above embodiments according to the technical essence of the invention, still Belong in the range of technical solution of the present invention.

Claims (4)

1. a kind of method that molten-salt growth method prepares bismuth titanates nanometer rods, it is characterised in that the following steps are included:
Step 1: titanium sulfate is made into aqueous solution, the concentration for adjusting the titanium ion in solution is 0.03~0.8mol/L；
Step 2: bismuth nitrate is dissolved in the dilute nitric acid solution that mass concentration is 5%, the concentration for adjusting the bismuth ion in solution is 0.04~1.0mol/L；
Step 3: bismuth nitrate solution made from step 2 and excessive potassium hydroxide aqueous solution are mixed, make mixed molten Liquid pH value is 14, obtains the oxyhydroxide precipitation solution of bismuth, this precipitation solution is mixed with titanium sulfate solution made from step 1 It closes, wherein the molar ratio of bismuth ion and titanium ion is 4:3, and mixed precipitation solution was surpassed with ultrasonic echography 20~40 minutes Frequency of sound wave is 1000~2000W, dries obtained precipitation solution to obtain presoma later；
Step 4: presoma made from step 3 and the solid sodium chloride as fused salt are fully ground, gained mixture is placed in In corundum crucible, then crucible is put into electric furnace, after keeping the temperature 1h~3h under the conditions of 820~950 DEG C, taken out, it is cooling；
Step 5: being dried after sample after cooling is cleaned with deionized water to get the bismuth titanates nanometer rods of well-crystallized are arrived.
2. the method that molten-salt growth method according to claim 1 prepares bismuth titanates nanometer rods, it is characterised in that ground in step 4 When presoma and sodium chloride weight ratio be 1:2~1:10.
3. the method that molten-salt growth method according to claim 1 prepares bismuth titanates nanometer rods, it is characterised in that the bismuth nitrate, It is pure that the purity of titanium sulfate and potassium hydroxide is not less than chemistry.
4. the method that molten-salt growth method according to claim 1 prepares bismuth titanates nanometer rods, it is characterised in that gained bismuth sodium titanate The length of rice stick is 300~600nm, and diameter is 30~80nm.
CN201811487968.6A 2018-12-06 2018-12-06 Method for preparing bismuth titanate nano-rod by molten salt method Active CN109336174B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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CN103466703A (en) * 2013-09-29 2013-12-25 安徽工业大学 Bismuth titanate nanoneedle and preparation method thereof
CN104211116A (en) * 2014-08-26 2014-12-17 浙江大学 Preparation method of Bi4Ti3O12 single-crystal nanorod and Bi4Ti3O12 single-crystal nanorod product
CN105645469A (en) * 2016-03-09 2016-06-08 武汉科技大学 Nano rodlike lanthanum titanate powder and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110281111A1 (en) * 2010-05-11 2011-11-17 Board Of Regents Of The Nevada System Of Higher Education, On Behalf Of The University Of Nevada, Synthesis of pyrochlore nanostructures and uses thereof
CN102531582A (en) * 2011-12-29 2012-07-04 洛阳理工学院 Method for preparing sodium bismuth titanate nanometer sheet
CN103466703A (en) * 2013-09-29 2013-12-25 安徽工业大学 Bismuth titanate nanoneedle and preparation method thereof
CN104211116A (en) * 2014-08-26 2014-12-17 浙江大学 Preparation method of Bi4Ti3O12 single-crystal nanorod and Bi4Ti3O12 single-crystal nanorod product
CN105645469A (en) * 2016-03-09 2016-06-08 武汉科技大学 Nano rodlike lanthanum titanate powder and preparation method thereof

Non-Patent Citations (2)

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Title
HAJIME WAGATA ET AL.: "Chloride Flux Growth of La2Ti2O7 Crystals and Subsequent Nitridation To Form LaTiO2N Crystals", 《CRYSTAL GROWTH & DESIGN》 *
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